CN102560270A - Pure steel spectrum standard sample and preparation method thereof - Google Patents
Pure steel spectrum standard sample and preparation method thereof Download PDFInfo
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 83
- 239000010959 steel Substances 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title abstract description 5
- 238000001228 spectrum Methods 0.000 title abstract description 5
- 238000004458 analytical method Methods 0.000 claims abstract description 31
- 238000005070 sampling Methods 0.000 claims abstract description 9
- 229910052729 chemical element Inorganic materials 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 230000003595 spectral effect Effects 0.000 claims description 8
- 238000012360 testing method Methods 0.000 claims description 6
- 241001417490 Sillaginidae Species 0.000 claims 1
- 238000005464 sample preparation method Methods 0.000 claims 1
- 238000003723 Smelting Methods 0.000 abstract description 14
- 238000005242 forging Methods 0.000 abstract description 6
- 238000003754 machining Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 26
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 9
- 238000007670 refining Methods 0.000 description 9
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- 238000004519 manufacturing process Methods 0.000 description 7
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- 238000005261 decarburization Methods 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
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- 229910052748 manganese Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
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- 229910052804 chromium Inorganic materials 0.000 description 4
- 238000009749 continuous casting Methods 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 238000006477 desulfuration reaction Methods 0.000 description 4
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- 229910052742 iron Inorganic materials 0.000 description 4
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- 239000000126 substance Substances 0.000 description 4
- 235000006679 Mentha X verticillata Nutrition 0.000 description 3
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- 241001062472 Stokellia anisodon Species 0.000 description 3
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- 238000001479 atomic absorption spectroscopy Methods 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
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- 229910000851 Alloy steel Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910000742 Microalloyed steel Inorganic materials 0.000 description 2
- 206010039509 Scab Diseases 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
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- 238000000540 analysis of variance Methods 0.000 description 2
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- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
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- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
- Treatment Of Steel In Its Molten State (AREA)
Abstract
The invention discloses a pure steel spectrum standard sample, which contains the following chemical elements in percentage by weight: c: 0.0017 to 0.0279, Si: 0.0100 to 0.0221, Mn: 0.118-0.271, P: 0.0067-0.0108, S: 0.0037-0.0056, Ni: 0.0021-0.0064, Cr: 0.0095-0.0176, Cu: 0.0030 to 0.0135, Ti: 0.0251 to 0.0649, Alt: 0.0014 to 0.0466, N: 0.00123-0.0030, and the balance of Fe element and inevitable impurities. The preparation method of the pure steel spectrum standard sample comprises the following steps: smelting and sampling; b, forging; c, machining by a lathe; d, inspecting uniformity; e, carrying out fixed value analysis on the characteristic quantity values to determine each characteristic quantity value.
Description
Technical field
The present invention relates to a kind of standard model of differentiating the elemental composition analysis of soft steel, micro-alloyed steel and Clean Steel process materials, particularly a kind of spectral standard sample of Clean Steel smelting technology.
Background technology
Along with the develop rapidly of world steel metallurgical technology, for satisfying the needs of market production high technology content and high value added product, iron and steel enterprise has all stepped into Clean Steel and Ultra-low carbon, large quantities of exploitations of micro-alloyed steel, production phase.Technical qualification and throughput that Clean Steel is smelted reach its maturity, and the content of P, C, S, O, N, H six big elements can be controlled at below 100ppm～120ppm.Can carry out assignment accurately to the element technical indicator of Clean Steel?---this problem has become the key problem of correct evaluation Clean Steel.Simultaneously production on-line analysis low levels, super low loading element technology have been proposed requirements at the higher level, this also is restriction Clean Steel production and realizes the important factor that the Clean Steel on-line analysis detects.
It is main with direct-reading spectrometer mainly that the Iron and Steel Production on-line analysis detects; Research detection department is equipped with means such as inductive coupling plasma emission spectrograph (ICP-AES), Atomic Absorption Spectroscopy AAS (AAS) and gas analyzer, but these analysis means all are the analytical instrument of detectability in the ppm level.There is the problem of several aspects in Clean Steel commercialization check: the one, and direct-reading spectrometer does not have the Clean Steel spectral standard sample to proofread and correct, and can't set up working curve to the super low loading element and carry out quantitative analysis; The 2nd, metallurgyization check industry has only low alloy steel and soft steel class standard sample at present; There is not standard model with the corresponding Clean Steel smelting technology of modern smelting technology; In the metallurgy check analysis, can only set up the method working curve of Clean Steel commercialization check analysis like this with low alloy steel or soft steel.Because the analysis of spark direct-reading spectrometer is a kind of relative spectrum relative method, has very big matrix effect, uses this class standard sample to cause reviewer's error in judgement easily, cause the Clean Steel series products to exist than mistake at X-ray inspection X.
Development Clean Steel standard model is set up quick, accurately analysis that Clean Steel On-line Product photoelectric direct reading spectrometry method realizes multielement, improves Clean Steel on-line analysis level and has become the task of top priority.
Summary of the invention
The object of the invention provides a kind ofly can verify the Clean Steel quality product, produces with the Clean Steel smelting technology, has spectral standard sample of C, Si, Mn, P, S, Cr, Ni, Cu, Alt and N characteristic of elements value and preparation method thereof.
The chemical element that all contains following weight per-cent in the Clean Steel standard sample for spectrochemical analysis steel among the present invention: C:0.0017～0.0279, Si:0.0100～0.0221, Mn:0.118～0.271; P:0.0067～0.0108, S:0.0037～0.0056, Ni:0.0021～0.0064; Cr:0.0095～0.0176, Cu:0.0030～0.0135, Ti:0.0251～0.0649; Alt:0.0014～0.0466, N:0.00123～0.0030, surplus is Fe element and inevitable impurity.
For realizing goal of the invention, the major technique operational path that the present invention adopts comprises: smelting, sampling → forging rolling → sample processing → standard specimen uniformity testing → standard specimen characteristic value are analyzed and are confirmed.
1, smelt, sampling: smelt hot metal pretreatment and the ladle refining means of adopting, the removal of detrimental impurity in the steel decomposed each operation, by C, H, O, N, P, S and inclusion content in the furnace outer refining technology control steel, pureization of assurance molten steel.
Clean Steel is smelted and to be taked main technique: hot metal pretreatment → converter → refining (ANS, RH, LF, VD) → continuous casting, and single according to continuously cast bloom chemistry material, obtain from continuously cast bloom and to meet standard model of the present invention and be developed into the pure steel billet appearance that the branch design requires.
3, forge: steel billet strips off the skin after bright and clean through lathe; Sawing machine is divided into fritter; Heat, forge and retarded cooling process: steel billet advances process furnace in room temperature and heats up, and heats up according to 800 ℃～1000 ℃～1200 ℃ three stepping row order ladder type, and each temperature platform was according to example weight insulation 1～2 hour; Forge 950 ℃～1150 ℃ of temperature, gradation forges, and prevents implosion; The steel billet cooling is taked to preheat sand drift and is buried cold slow cooling technology.Forge sample requirement pole surface, back flawless, scab, do not have and mix appearance, diameter is in Φ 45mm ± 2mm scope, and the pole of long 800mm～1000mm, pole are directly spent error can not surpass 1.5mm.
4, machined into: with diameter of phi 45mm up-to-standard behind the forging rolling ± 2mm; The pole sample of long 800mm～1000mm strips off the skin through lathe---sawing machine stripping and slicing---lathe chamfered edge---polishing---alcohol wash moisture (control is got rusty); Finally being processed into Φ 38mm * 30mm bulk sample, promptly is last standard model.
5, uniformity testing: select Elements C, Si, Mn, P, S, N, Ni, Cr, Cu, the Al composition of main definite value project and easy segregation, poor stability to carry out uniformity testing, the analysis of variance that adopts F to check is represented the homogeneity of sample.
6, adopt two or more different principle analytical procedures to carry out the definite value analysis of characteristic value jointly by eight tame laboratories, combined data, mathematical statistics are confirmed each characteristic value.
Clean Steel standard specimen composition of the present invention is designed to 6 serial Clean Steel standard models, and the characteristic of elements value has the linear dependence more than 3, and relation conefficient is seen accompanying drawing more than 0.99.The chemical element linearity range is wide, covers whole steel grades in the Clean Steel smelting technology, uses applicable to the spectrum analyzer mass analysis of various Clean Steel handicraft products such as IF, pipeline, cord.Sample is smelted owing to adopted the Clean Steel refinery practice; Clean Steel heating, the gentle refrigeration technique of forging significantly improve standard specimen chemical ingredients homogeneity, and have improved processing characteristics; Through the COMAR retrieval, the good uniformity of standard model of the present invention is in similar domestic and import standard model.
Through taking above technical scheme, the present invention has following beneficial effect:
1, owing to adopted the Clean Steel smelting technology of hot metal pretreatment → converter → refining (ANS, RH, LF, VD) → continuous casting, the chemical ingredients of Clean Steel standard model of the present invention is even, dense structure; Owing to adopt rational forging process and retarded cooling process, significantly improve standard specimen chemical ingredients homogeneity again;
2, the spectroscopic analysis of this Clean Steel is to transmit " measurement instrument " that corresponding Clean Steel series products becomes component value with the characteristic value of the determined C of national standard sample, Si, Mn, P, S, Cr, Ni, Cu, Alt and N.This patent product application is set up analytical procedure and working curve in direct-reading spectrometer; It is online modified to realize that the Clean Steel smelting is produced, and controlled on-line that realizes the Clean Steel quality of production and the on-line analysis insolation level that improves Clean Steel production are had great promoter action.
Description of drawings
Fig. 1 is the linear fitted figure of Clean Steel standard sample for spectrochemical analysis C element;
Fig. 2 is the linear fitted figure of Clean Steel standard sample for spectrochemical analysis Si element;
Fig. 3 is the linear fitted figure of Clean Steel standard sample for spectrochemical analysis Mn element;
Fig. 4 is the linear fitted figure of Clean Steel standard sample for spectrochemical analysis P element;
Fig. 5 is the linear fitted figure of Clean Steel standard sample for spectrochemical analysis S element;
Fig. 6 is the linear fitted figure of Clean Steel standard sample for spectrochemical analysis Ni element;
Fig. 7 is the linear fitted figure of Clean Steel standard sample for spectrochemical analysis Cr element;
Fig. 8 is the linear fitted figure of Clean Steel standard sample for spectrochemical analysis Cu element;
Fig. 9 is the linear fitted figure of Clean Steel standard sample for spectrochemical analysis Al element.
Embodiment
Below in conjunction with embodiment the present invention is further specified:
The present invention further specifies summary of the invention through embodiment, but not limit by embodiment.
Clean Steel spectral standard sample of the present invention comprises 6 points, and the weight percent of each point component concentration sees the following form:
The total weight percent summary sheet of Clean Steel standard sample for spectrochemical analysis CJG1#～CJG6# chemical element (ω %)
| Numbering | Project | C | Si | Mn | P | S | Ni | Cr |
| CJG-1# | Standard value | 0.0023 | 0.0158 | 0.183 | 0.0083 | 0.0042 | 0.0021 | 0.0151 |
| CJG-2# | Standard value | 0.0017 | 0.0221 | 0.172 | 0.0078 | 0.0037 | 0.0064 | 0.0168 |
| CJG-3# | Standard value | 0.0019 | 0.0168 | 0.148 | 0.0082 | 0.0045 | 0.0031 | 0.0176 |
| CJG-4# | Standard value | 0.0034 | 0.0170 | 0.118 | 0.0067 | 0.0056 | 0.0063 | 0.0095 |
| CJG-5# | Standard value | 0.0042 | 0.0188 | 0.155 | 0.0091 | 0.0045 | 0.0035 | 0.0174 |
| CJG-6# | Standard value | 0.0279 | 0.0100 | 0.271 | 0.0108 | 0.0038 | 0.0035 | 0.0166 |
| Numbering | Project | Cu | Ti | Al t | N | ? | ? | ? |
| CJG-1# | Standard value | 0.0030 | 0.0649 | 0.0466 | 0.00130 | ? | ? | ? |
| CJG-2# | Standard value | 0.0135 | 0.0704 | 0.0447 | 0.00123 | ? | ? | ? |
| CJG-3# | Standard value | 0.0033 | 0.0362 | 0.0014 | 0.00269 | ? | ? | ? |
| CJG-4# | Standard value | 0.0081 | 0.0564 | 0.0192 | 0.00003 | ? | ? | ? |
| CJG-5# | Standard value | 0.0032 | 0.0251 | 0.0015 | 0.00002 | ? | ? | ? |
| CJG-6# | Standard value | 0.0056 | 0.0205 | 0.0232 | 0.00153 | ? | ? | ? |
The preparation method of the above-mentioned Clean Steel spectral standard sample of invention is characterized in that it is
Undertaken by following step:
1, smelt, take a sample:
Smelting technology is taked the Clean Steel smelting technology of hot metal pretreatment → converter → refining (ANS, RH, LF, VD) → continuous casting.
2, Clean Steel is smelted the control techniques measure of elemental composition:
2.1 super low sulfur control techniques
Ultralow-sulfur steel operational path: molten iron pretreatment desulfurizing-converter smelting-steel secondary refining desulfurization
To S content control from hot metal pretreatment desulfurization just, converter suppresses back sulphur, each link of the dark desulfurization of refining is all taked measure of control: hot metal pretreatment (CaO+Mg) realization molten iron S content≤20 * 10-6; Converter control molten steel returns sulphur≤30 * 10-6; Refining realizes LF, CAS-OB, the dark desulfurization of VD.
2.2 Ultra-low carbon control techniques: RH-TB decarburization technique
2.2.1RH decarburization technique comprises 2 points: Composition Control before the decarburization and acceleration RH decarburization technique.
(1) Composition Control before the decarburization: Clean Steel is smelted the top and bottom complex blowing smelting suprelow carbon steel and is taked omnidistance blowing argon gas, and the phase bottom blowing gas intensity is respectively 0.06,0.04 and 0.08Nm before, during and after the smelting
3/ mint.
(2) quicken the RH decarburization technique: through increasing the converter gas flow from 2Nm
3/ mint rises to 15Nm
3/ mint, thus the circular flow of molten steel in the increase RH-TB effectively quickens decarbonization rate, the minimum 10ppm that reduces to of carbon.
2.2.2 prevent molten steel recarburization technology: adopt no carbon refractory and various slag agent to prevent that solidification of molten steel from becoming in the strand process, the carburetting that contacts of molten steel and carbonaceous lining ladle brick, long nozzle and covering slag, the whole process carbon increasing amount is controlled at about 3ppm.
2.3 T [O] is controlled major measure: control converter terminal [C] * [O]≤0.0029.Take measures to reducing the ladle top slag modification technology of ladle top slag oxidisability, Si, Mn, Al, Al-Mg, Ti complex deoxidization technology.
2.4 to N content control mainly from denitrogenation with prevent two aspects considerations of nitrogen pick-up: VD vacuum outgas treatment technology; Converter tapping control nitrogen and protection casting technique.
2.5 to P content major control measure: adopt the ARP technology; Converter " two slag " dephosphorizing technology with prevent molten steel rephosphorization control techniques.
2.6H content control: optimize refractory materials baking process, ladle, the mouth of a river; Go into the control of stove alloy and slag making materials; VD, the RH vacuum-treat degassing.
2.7 metallographic structure check: sampling, carry out inclusion and metallographic structure check, specimen holder foreign material rank is all in standard range, and dense structure, even.
2.8 sampling: singly choosing with control P, S constituent content through stokehold chemical examination material earlier is master's sample; Control N≤30ppm; Converter refining target [C]+[S]≤50ppm; Other microalloy elements consider to select sampling from the Gradient distribution angle, on the basis of a large amount of samplings, replenish vacuum induction furnace smelting, and the content that screens or adjust trace elements is to reach the purpose of each element distribution gradient.
Through the chemical element initial survey, the continuous casting working procedure sampling obtains and definite six steel billets that meet the design of Clean Steel standard specimen composition, as Clean Steel standard specimen development appearance.Selected strand appearance, specification 230 * 240 * 1000 (mm), the heavily about 350Kg of blank.
3, forge: steel billet strips off the skin after bright and clean through lathe; Sawing machine is divided into fritter; Heat, forge and retarded cooling process: steel billet advances process furnace in room temperature and heats up, and heats up according to 800 ℃～1000 ℃～1200 ℃ three stepping row order ladder type, and each temperature platform was according to example weight insulation 1～2 hour; Forge 950 ℃～1150 ℃ of temperature, gradation forges, and prevents implosion; The steel billet cooling is taked to preheat sand drift and is buried cold slow cooling technology.Forge the back sample diameter in Φ 45mm ± 2mm scope, the pole of long 800mm～1000mm, pole are directly spent error and are no more than 1.5mm, and pole surface flawless, scab, do not have and mix kind.
4, machined into: with diameter of phi 45mm up-to-standard behind the forging rolling ± 2mm; The pole sample of long 800mm～1000mm strips off the skin through lathe---sawing machine stripping and slicing---lathe chamfered edge---polishing---alcohol wash moisture (control is got rusty); Finally being processed into Φ 38mm * 30mm bulk sample, promptly is last standard model.
5, uniformity testing: the element of selecting main definite value project and easy segregation, poor stability: C, Si, Mn, P, S, N, Ni, Cr, Cu, V, Al composition carry out uniformity testing, and the analysis of variance that adopts F to check is represented the homogeneity of sample.
6, adopt two or more different principle analytical procedures to carry out the definite value analysis of characteristic value jointly by eight tame laboratories, combined data, mathematical statistics are confirmed each characteristic value.
The element definite value analytical procedure of taking gathers as follows.
Claims (2)
1. Clean Steel spectral standard sample contains the chemical element of following weight per-cent: C:0.0017～0.0279, Si:0.0100～0.0221, Mn:0.118～0.271; P:0.0067～0.0108, S:0.0037～0.0056, Ni:0.0021～0.0064; Cr:0.0095～0.0176, Cu:0.0030～0.0135, Ti:0.0251～0.0649; Alt:0.0014～0.0466, N:0.00123～0.0030, surplus is Fe element and inevitable impurity.
2. a Clean Steel spectral standard sample preparation method according to claim 1 is characterized in that comprising the steps: that a smelts, sampling; B forges; The c machined into; The d uniformity testing; E carries out the definite value analysis of characteristic value, confirms each characteristic value.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103115870A (en) * | 2013-01-28 | 2013-05-22 | 青岛云路新能源科技有限公司 | Laboratory preparation method of iron-base amorphous spectral standard sample |
| CN106282748A (en) * | 2016-08-30 | 2017-01-04 | 河钢股份有限公司 | The production method of silicon steel spectral standard sample steel |
| CN106282773A (en) * | 2016-08-30 | 2017-01-04 | 河钢股份有限公司 | The production method of low-sulfur steel spectrum analysis standard specimen steel |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410572A (en) * | 2002-10-01 | 2003-04-16 | 西南铝业（集团）有限责任公司 | High silicon cast aluminium spectrum standard sample and its preparation method |
| CN1696637A (en) * | 2005-05-20 | 2005-11-16 | 东北轻合金有限责任公司 | Spectrum of aluminum alloy, Chemical standard specimen, and preparation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410572A (en) * | 2002-10-01 | 2003-04-16 | 西南铝业（集团）有限责任公司 | High silicon cast aluminium spectrum standard sample and its preparation method |
| CN1696637A (en) * | 2005-05-20 | 2005-11-16 | 东北轻合金有限责任公司 | Spectrum of aluminum alloy, Chemical standard specimen, and preparation method |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103115870A (en) * | 2013-01-28 | 2013-05-22 | 青岛云路新能源科技有限公司 | Laboratory preparation method of iron-base amorphous spectral standard sample |
| CN106282748A (en) * | 2016-08-30 | 2017-01-04 | 河钢股份有限公司 | The production method of silicon steel spectral standard sample steel |
| CN106282773A (en) * | 2016-08-30 | 2017-01-04 | 河钢股份有限公司 | The production method of low-sulfur steel spectrum analysis standard specimen steel |
| CN106282773B (en) * | 2016-08-30 | 2018-02-23 | 河钢股份有限公司 | The production method of low-sulfur steel spectrum analysis standard specimen steel |
| CN106282748B (en) * | 2016-08-30 | 2018-02-23 | 河钢股份有限公司 | The production method of silicon steel spectral standard sample steel |
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